CN102061481B - Surface pulse electroplated Ni-Si composite coating of normal cold rolled steel sheet and hot atom infiltration treatment method thereof - Google Patents

Surface pulse electroplated Ni-Si composite coating of normal cold rolled steel sheet and hot atom infiltration treatment method thereof Download PDF

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CN102061481B
CN102061481B CN2010105882819A CN201010588281A CN102061481B CN 102061481 B CN102061481 B CN 102061481B CN 2010105882819 A CN2010105882819 A CN 2010105882819A CN 201010588281 A CN201010588281 A CN 201010588281A CN 102061481 B CN102061481 B CN 102061481B
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rolled steel
steel sheet
retention
cold rolled
plating bath
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CN102061481A (en
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钟庆东
杜海龙
盛敏奇
王毅
李振华
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State Grid Shanghai Electric Power Co Ltd
University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Abstract

The invention relates to a surface pulse electroplated Ni-Si composite coating of the normal cold rolled steel sheet and a hot atom infiltration treatment method thereof, and belongs to the technical field of metal surface alloying treatment. The invention is characterized in that: a Ni-Si composite coating is induced by using nanosilicon powder by a pulse electroplating method; and the Ni-Si composite coating infiltrates into the surface of the cold rolled steel sheet under a reducing atmosphere by high-temperature hot atom infiltration treatment. The corrosion resistance of the normal cold rolled steel sheet treated by the method is obviously improved, the coating of the cold rolled steel sheet has high bonding force, high salt resistance and high acid resistance, and the corrosion current density of the coating is obviously reduced.

Description

The treatment process that common surface of cold-rolled steel plate pulse plating Ni-Si composite deposite and retention thereof ooze
Technical field
The present invention relates to the treatment process that a kind of common cold-reduced sheet surface pulse plating Ni-Si composite deposite and retention thereof ooze.Belong to the metal surface alloy processing technology field.
In chemical industry, because the requirement on producing, chemical plant has etching problem inevitably and produces.Bring thus except such as financial losses such as changing device, equipment parking, product loss more, that even more serious then is is damaged owing to equipment, blast endangers personnel safety, and the environmental pollution that leakage caused and the wasting of resources of raw material, product.At present, common equipment anticorrosion technology has reasonable material, surface protection (comprising metal plating and Fei Jin layer coating), and surrounding medium is handled, electro-chemical protection and protection against corrosion design etc.
Plating work is carried out relatively early, has and has gone up century-old history, has obtained significant progress in recent years, especially aspect decorative electroplating, has obtained gratifying achievement, like imitation gold plating.Along with national defense industry, automotive industry and transmission of electricity industrial expansion; People require increasingly high to the solidity to corrosion of plated item; The simple zinc-plated needs that can not satisfy high anti-corrosion, therefore, composite plating has leapt to people's the visual field gradually; Composite plating be through electrodip process with a kind of or several insoluble solid particulates, be mingled with in the metal plating method that forms property coating equably.It is good to find that after deliberation zn-ni alloy deposits has solidity to corrosion, outward appearance light characteristic not easy to fade.The zn-ni alloy deposits of nickel content 8 %～13 % has the solidity to corrosion than 7～10 times of zinc-plated floor heights, the zn-ni alloy deposits outward appearance behind chromatic passivation can keep 10 years constant.Zn-ni alloy deposits does not have hydrogen embrittlement, and the protective that especially is fit to spring part, standardized component is electroplated.Zn-ni alloy deposits still can provide favorable protection property after bakingout process, deformation processing and other processing.
Electroplating Ni – SiC composite deposite is good, anti-oxidant, the corrosion resistant composite deposite of a kind of high firmness, wear resisting property, is widely used in parts such as mould, measurer, engine cylinder.This paper adopts orthogonal experiment to inquire into different technical parameters to the composite deposite Effect on Performance through processing parameters such as control nanometer Si powder particle suspension amount, cathode current density, temperature, pH, stir speed (S.S.)s, has drawn optimum process scheme.Through these methods, the etching problem in the chemical plant has obtained certain solution.But the etching problem of reductant (especially cl ions) is perplexing scientific research, the producers of chemical plant and metallurgy industry always.Though because Hastelloy, duplex stainless steel have corrosion stability preferably to cl ions, price is very expensive, is difficult to large-scale promotion, then usually effect is little when addressing this problem for general stainless steel.
As far back as nineteen fifty, Brenner A just uses electrodip process to obtain amorphous phosphorus-nickel alloy.Because it not only has excellent corrosion resisting property, and after heat treatment, its hardness and wear resistance can compare favourably with durionise, thereby receives extensive concern.Four during the last ten years, and both at home and abroad the scientific research personnel has done a large amount of work at the phase structure and the aspects such as measuring method, coating performance and corrosion resistance mechanism of bath element and plating condition, mechanism of electrodeposition and non-crystalline state formation condition, coating.
Summary of the invention
The purpose of this invention is to provide a kind of treatment process of oozing at common surface of cold-rolled steel plate pulse plating Ni-Si composite deposite and retention thereof.
The present invention is the treatment process that a kind of common surface of cold-rolled steel plate pulse plating Ni-Si composite deposite and retention thereof ooze, and it is characterized in that having following process and step:
The pre-treatment of a cold-rolled steel sheet: the common cold-rolled steel sheet that desire is handled is through alkali cleaning, pickling, washing, and dry back is subsequent use;
B prepares plating bath: the raw material composition and the volume mass content thereof of plating bath are following:
NiCl 2·6H 2O 25～50g/L
NiSO 4·6H 2O 100～150g/L
H 3BO 3 30～40g/L
C 6H 8O 7·6H 2O 10～12g/L
NH 4HF 2 10～15g/L
Polyoxyethylene glycol 2～10g/L
Nanometer Si powder 10～50g/L
C electroplates: put into above-mentioned plating bath through pretreated common cold-rolled steel sheet and electroplate above-mentioned, the pH value of electroplate liquid is adjusted to 2.5-5.8; The temperature of plating bath is 30-60 OC; The anode that adopts is a nickel electrode; Electroplating time is 20～30 minutes.
Current parameters is: average current density 0.8～-1.5A/dm 2, peak current density 5～7A/ dm 2, the break make ratio 200 μ s:200 μ s～200 μ s:600 μ s in burst length;
D carries out retention to composite deposite and oozes processing: this process of thermal treatment parameter is following:
Retention oozes temperature: 500-800 OC
H 2Air flow is: 1L/min---3L/min
Heating gradient: 5--10 OC/min
Soaking time: 2---5h
Cooling gradient: 10--30 OC/min
Characteristics of the present invention and advantage are narrated as follows: the heat treating method that pulse plating that adopts among the present invention and retention ooze can strengthen the corrosion resistance nature of common cold-rolled steel sheet effectively; And owing to added an amount of nano silica fume, make it form Ni-Si composite alloy coating, help improving corrosion resistance nature.Also adopted feeding H in addition 2Carry out the heat treating method that retention oozes, at H 2The reducing atmosphere condition under, make partial oxide reduction and can guarantee that retention can stable existence, the infiltration of retention can improve the corrosion resistance nature of composite deposite.
Embodiment
After practical implementation of the present invention being described at present.
Embodiment 1
The process and the step of present embodiment are following:
(1) the cleaning pre-treatment of cold-rolled steel sheet sample.
(2) preparation Essential Chemistry plating bath: NiCl 26H 2O 35g/L, NiSO 46H 2O 120g/L, H 3BO 335g/L, C 6H 8O 76H 2O 10g/L, NH 4HF 211 g/L, tensio-active agent (polyoxyethylene glycol) 5g/L, adjustment pH value is 4.5, temperature is controlled at 20 OC adds the nanometer Si powder behind the 10 g/L ball millings.
(3) sample that pre-treatment is good immerses and electroplates in the plating bath after 15 minutes, takes out.
(4) composite deposite is carried out retention and ooze, its processing parameter is: retention oozes temperature: 500-800 OC, H 2Air flow is: 1L/min---3L/min, heating gradient: 5--10 OC/min, soaking time: 2---5h, cooling gradient: 10--30 OC/min
Salt mist experiment is carried out on common cold-reduced sheet surface passing through after plating and retention ooze processing, records salt-fog resistant time; Be soaked in simultaneously in 5% metabisulfite solution behind the 30min, test its polarization curve, draw its corrosion electric current density.
Electro-chemical test adopts three-electrode system, and reference electrode is a SCE, and counter electrode is the Pt electrode, is soaked into the 5%Na by AR and deionized water preparation with above-mentioned through pretreatment sample 2SO 4In the solution, be to carry out the polarization curve test on the electrochemical workstation of CHI660C in model.
Embodiment 2
The process and the step of present embodiment are following:
(1) the cleaning pre-treatment of cold-rolled steel sheet sample
(2) preparation Essential Chemistry plating bath: NiCl 26H 2O 35g/L, NiSO 46H 2O 120g/L, H 3BO 335g/L, C 6H 8O 76H 2O 10g/L, NH 4HF 211 g/L, tensio-active agent (polyoxyethylene glycol) 5g/L, adjustment pH value is 4.5, temperature is controlled at 30 OC adds the nanometer Si powder behind the 20 g/L ball millings.
(3) sample that pre-treatment is good immerses and electroplates in the plating bath after 15 minutes, takes out.
(4) composite deposite is carried out retention and ooze, its processing parameter is: retention oozes temperature: 500-800 OC, H 2Air flow is: 1L/min---3L/min, heating gradient: 5--10 OC/min, soaking time: 2---5h, cooling gradient: 10--30 OC/min
Salt mist experiment is carried out on common cold-reduced sheet surface passing through after plating and retention ooze processing, records salt-fog resistant time; Be soaked in simultaneously in 5% metabisulfite solution behind the 30min, test its polarization curve, draw its corrosion electric current density.
Electro-chemical test adopts three-electrode system, and reference electrode is a SCE, and counter electrode is the Pt electrode, is soaked into the 5%Na by AR and deionized water preparation with above-mentioned through pretreatment sample 2SO 4In the solution, be to carry out the polarization curve test on the electrochemical workstation of CHI660C in model.
Embodiment 3
The process and the step of present embodiment are following:
(1) the cleaning pre-treatment of cold-rolled steel sheet sample
(2) preparation Essential Chemistry plating bath: NiCl 26H 2O 35g/L, NiSO 46H 2O 120g/L, H 3BO 335g/L, C 6H 8O 76H 2O 10g/L, NH 4HF 211 g/L, tensio-active agent (polyoxyethylene glycol) 5g/L, adjustment pH value is 4.5, temperature is controlled at 40 OC adds the nanometer Si powder behind the 30 g/L ball millings.
(3) sample that pre-treatment is good immerses and electroplates in the plating bath after 15 minutes, takes out.
(4) composite deposite is carried out retention and ooze, its processing parameter is: retention oozes temperature: 500-800 OC; H 2Air flow is: 1L/min---3L/min; Heating gradient: 5--10 OC/min; Soaking time: 2---5h, cooling gradient: 10--30 OC/min.
Salt mist experiment is carried out on common cold-reduced sheet surface passing through after plating and retention ooze processing, records salt-fog resistant time; Be soaked in simultaneously in 5% metabisulfite solution behind the 30min, test its polarization curve, draw its corrosion electric current density.
Electro-chemical test adopts three-electrode system, and reference electrode is a SCE, and counter electrode is the Pt electrode, is soaked into the 5%Na by AR and deionized water preparation with above-mentioned through pretreatment sample 2SO 4In the solution, be to carry out the polarization curve test on the electrochemical workstation of CHI660C in model.
Embodiment 4
The process and the step of present embodiment are following:
(1) the cleaning pre-treatment of cold-rolled steel sheet sample
(2) preparation Essential Chemistry plating bath: NiCl 26H 2O 35g/L, NiSO 46H 2O 120g/L, H 3BO 335g/L, C 6H 8O 76H 2O 10g/L, NH 4HF 211 g/L, tensio-active agent (polyoxyethylene glycol) 5g/L, adjustment pH value is 4.5, temperature is controlled at 50 OC adds the nanometer Si powder behind the 40 g/L ball millings.
(3) sample that pre-treatment is good immerses and electroplates in the plating bath after 15 minutes, takes out.
(4) composite deposite is carried out retention and ooze, its processing parameter is: retention oozes temperature: 500-800 OC, H 2Air flow is: 1L/min---3L/min, heating gradient: 5--10 OC/min, soaking time: 2---5h, cooling gradient: 10--30 OC/min
Salt mist experiment is carried out on common cold-reduced sheet surface passing through after plating and retention ooze processing, records salt-fog resistant time; Be soaked in simultaneously in 5% metabisulfite solution behind the 30min, test its polarization curve, draw its corrosion electric current density.
Electro-chemical test adopts three-electrode system, and reference electrode is a SCE, and counter electrode is the Pt electrode, is soaked into the 5%Na by AR and deionized water preparation with above-mentioned through pretreatment sample 2SO 4In the solution, be to carry out the polarization curve test on the electrochemical workstation of CHI660C in model.
Electro-chemical test adopts three-electrode system, and reference electrode is a SCE, and counter electrode is the Pt electrode, and electrode to be measured is soaked into the 5%Na by AR and deionized water preparation 2SO 4In the solution, be to carry out the polarization curve test on the electrochemical workstation of CHI660C in model.
Comparative Examples
Among this comparative example, in plating bath, add the nano-silicon powder.
Treating processes and step are following:
Preparation Essential Chemistry plating bath: NiCl 26H 2O 35g/L, NiSO 46H 2O 120g/L, H 3BO 335g/L, C 6H 8O 76H 2O 10g/L, NH 4HF 211 g/L, tensio-active agent (polyoxyethylene glycol) 5g/L, adjustment pH value is 4.5, temperature is controlled at 60 OC does not add nanometer Si powder.The sample that pre-treatment is good immerses to be electroplated in the plating bath after 15 minutes, took out.
Composite deposite is carried out retention ooze, its processing parameter is: retention oozes temperature: 500-800 OC, H 2Air flow is: 1L/min---3L/min, heating gradient: 5--10 OC/min, soaking time: 2---5h, cooling gradient: 10--30 OC/min
Salt mist experiment is carried out on common cold-reduced sheet surface passing through after plating and retention ooze processing, records salt-fog resistant time; Be soaked in simultaneously in 5% metabisulfite solution behind the 30min, test its polarization curve, draw its corrosion electric current density.
Electro-chemical test adopts three-electrode system, and reference electrode is a SCE, and counter electrode is the Pt electrode, is soaked into the 5%Na by AR and deionized water preparation with above-mentioned through pretreated sample 2SO 4In the solution, be to carry out the polarization curve test on the electrochemical workstation of CHI660C in model
In the various embodiments described above, adopted different nano silica fume body burdens, final experimental result is shown in the following table 1.
The different nano-powder content of table 1 are to cold-reduced sheet surface heat infiltration layer effect on corrosion
Nanometer Si powder content g/L Corrosion electric current density i (A/m 2） Salt-fog test (h)
0 3.5×10 -5 1630
10g/L 6.7×10 --6 1820
20g/L 2.1×10 -6 2000
30g/L 1.3×10 -5 1932
40g/L 5.6×10 -5 1911
Instance proves that the corrosion electric current density of the common surface of cold-rolled steel plate of utilizing technical finesse of the present invention is lower, and the salt-fog test time is longer, explains through surface treatment method of the present invention its corrosion resistance nature is improved greatly.

Claims (1)

1. treatment process that common cold-reduced sheet surface adopts pulse plating Ni-Si composite deposite and retention thereof to ooze is characterized in that having following process and step:
A. the pre-treatment of cold-rolled steel sheet: the common cold-rolled steel sheet that desire is handled is through alkali cleaning, pickling, washing, and dry back is subsequent use;
B. prepare plating bath: the raw material composition and the content thereof of plating bath are following:
NiCl 2·6H 2O 25～50g/L
NiSO 4·6H 2O 100～150g/L
H 3BO 3 30～40g/L
C 6H 8O 7·6H 2O 10～12g/L
NH 4HF 2 10～15g/L
Polyoxyethylene glycol 2～10g/L
Nanometer Si powder 10～50g/L
C. electroplate: put into above-mentioned plating bath through pretreated common cold-rolled steel sheet and electroplate above-mentioned, the pH value of electroplate liquid is adjusted to 2.5-5.8; The temperature of plating bath is 30-60 OC; The anode that adopts is a nickel electrode; Electroplating time is 20～30 minutes;
Current parameters is: average current density 0.8～-1.5A/dm 2, peak current density 5～7A/ dm 2, the break make ratio 200 μ s:200 μ s～200 μ s:600 μ s in burst length;
D. composite deposite is carried out retention and ooze processing: this process of thermal treatment parameter is following:
Retention oozes temperature: 500～800 OC
H 2Air flow is: 1L/min～3L/min
Heating gradient: 5～10 OC/min
Soaking time: 2～5h
Cooling gradient: 10～30 OC/min.
CN2010105882819A 2010-12-15 2010-12-15 Surface pulse electroplated Ni-Si composite coating of normal cold rolled steel sheet and hot atom infiltration treatment method thereof Active CN102061481B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1122118C (en) * 1997-07-04 2003-09-24 日本普莱泰克株式会社 Method of making iron-electroplated aluminium materials
CN1831204A (en) * 2005-03-08 2006-09-13 上海艾比西材料科技有限公司 Method and equipment for electroplating superthick and multiple-hole metals

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1122118C (en) * 1997-07-04 2003-09-24 日本普莱泰克株式会社 Method of making iron-electroplated aluminium materials
CN1831204A (en) * 2005-03-08 2006-09-13 上海艾比西材料科技有限公司 Method and equipment for electroplating superthick and multiple-hole metals

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